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机构地区:[1]广东药学院药科学院,广东广州510006 [2]广东省食品药品检验所,广东广州510180
出 处:《分析测试学报》2015年第9期1008-1013,共6页Journal of Instrumental Analysis
基 金:广东省省级科技计划项目(2013B090200059);广东省中医药局课题(20132110);广州市健康产品非法添加化学成分快速检测技术重点实验室项目(2013年)
摘 要:采用亚3μm色谱柱建立了同时快速检测腌腊肉制品中20种非法添加合成色素的高效液相色谱法。样品经石油醚脱脂、乙醇-氨水-水(7∶2∶1)提取、钨酸钠溶液沉淀蛋白,采用Agilent Poroshell 120 EC C18(50 mm×4.6 mm,2.7μm)色谱柱以甲醇-0.02 mol/L乙酸铵(p H 5.5)为流动相梯度洗脱,二极管阵列检测器检测,外标法定量。结果表明,待测物可在17 min内实现完全分离。20种成分的质量浓度在0.15~20.0 mg/L范围内与峰面积呈线性关系,相关系数(r)大于0.998,方法的回收率为70.3%~107.9%,相对标准偏差(RSD)为0.5%~3.1%,检出限为0.1~0.2 mg/kg。与传统5μm色谱柱ACE C18(250 mm×4.6 mm,5μm)相比,本方法节约了62%的分析时间,并能在常规HPLC系统内使用,具有广阔的应用前景。A rapid method was developed for the simultaneous determination of 20 synthetic colors in cured meat products by high performance liquid chromatography( HPLC) with sub- 3 μm columns.The samples were degreased with petroleum benzin,extracted with ethanol- ammonium hydroxide-water( 7 ∶ 2 ∶ 1) and deproteinized with sodium tungstate solution. The target compounds were separated on an Agilent Poroshell 120 EC C18column( 50 mm × 4. 6 mm,2. 7 μm) using methanol-0. 02 mol/L ammonium acetate solution( p H 5. 5) as mobile phase with gradient elution,and detected with DAD. The quantification analysis of analytes was performed by the external standard method. The result indicated that 20 analytes were separated completely in 17 min,and their calibration curves were linear in the range of 0. 15- 20. 0 mg/L with correlation coefficients more than 0. 998.The average recoveries at three spiked levels ranged from 70. 3% to 107. 9% with RSDs( n = 6) of0. 5%- 3. 1%. The detection limits were in the range of 0. 1- 0. 2 mg/kg. The method approximately reduced assay time by 62% compared with that of the regular ACE C18column( 250 mm × 4. 6mm,5 μm). The method could be performed routinely on a conventional LC system,which indicates an extensive application prospect.
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